Workflows Optimized for High Throughput, Robust Persistent Organic Pollutants (POPs) Analysis in Environmental Matrices

New Organic Monitoring Techniques
Oral Presentation

Prepared by R. Addink1, D. Walker2
1 - Fluid Management Systems, 900 Technology Park Drive, Billerica, MA, 01862, United States
2 - Agilent Technologies, 5301 Stevens Creek Blvd, Santa Clara, CA, 95051, United States

Contact Information: [email protected]; 617-393-2396


Persistent organic pollutants (POPs) such as polychlorinated dibenzo-p-dioxins (PCDDs), furans (PCDFs) and biphenyls (PCBs) have been a major environmental concern for a number of decades. Due to their low solubility in water and their resistance to breakdown, they tend to accumulate in river sediment. Analyses of sediment samples using US EPA methods 1613B (PCDD/Fs) and 1668C (PCBs) have been carried out around the world. Study of sediments often involves large amounts of samples, making fast processing (extraction, clean up, analysis) all the more important. This presentation describes workflows optimized using Automated Pressurized Liquid Extraction (PLE) and Semi Automated Sample column cleanup of river sediment. Quick and easy processing results in samples being ready in the same day using a Triple Quadrupole GC/MS

1g of sample was mixed with Hydromatrix® and spiked with 13C labeled standards. Samples were put in extraction cells. Pressurized Liquid Extraction with 50%/50% v/v dichloromethane/hexane (120oC, 1500psi, 20min) was carried out. Cleanup was done with semi-automated column chromatography, using high-capacity acid silica, alumina and carbon/celite columns. Solvents used were hexane, dichloromethane and toluene. Samples were analyzed using an alternate testing protocol for EPA 1613B using a Triple Quadrupole GC/MS.

13C PCDD/F recoveries varied between 82%-105% and between 93%-125% for PCBs. A certified reference sample of NIST river sediment with known composition was analyzed. Excellent agreement was found between native values of both PCDD/F and PCBs measured and the reference values provided.

Extraction, clean up and analysis by properly trained personnel can be carried out in one day, resulting in low turnaround times.